DE69030327T2 - Nitrogen manufacturing process - Google Patents

Nitrogen manufacturing process

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Publication number
DE69030327T2
DE69030327T2 DE69030327T DE69030327T DE69030327T2 DE 69030327 T2 DE69030327 T2 DE 69030327T2 DE 69030327 T DE69030327 T DE 69030327T DE 69030327 T DE69030327 T DE 69030327T DE 69030327 T2 DE69030327 T2 DE 69030327T2
Authority
DE
Germany
Prior art keywords
column
nitrogen
mixture
enriched
turbine
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
DE69030327T
Other languages
German (de)
Other versions
DE69030327D1 (en
Inventor
Sophie Gastinne
Bao Ha
Francois Venet
Naohiko Yamashita
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
Teisan KK
Air Liquide Process and Construction Inc
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Filing date
Publication date
Application filed by Air Liquide SA, Teisan KK, Air Liquide Process and Construction Inc filed Critical Air Liquide SA
Publication of DE69030327D1 publication Critical patent/DE69030327D1/en
Application granted granted Critical
Publication of DE69030327T2 publication Critical patent/DE69030327T2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
    • F25J3/04393—Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04296—Claude expansion, i.e. expanded into the main or high pressure column
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    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
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    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F25J3/04357—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen and comprising a gas work expansion loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/044—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a single pressure main column system only
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
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    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
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    • F25J3/04472—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages
    • F25J3/04496—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages for compensating variable air feed or variable product demand by alternating between periods of liquid storage and liquid assist
    • F25J3/04503—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages for compensating variable air feed or variable product demand by alternating between periods of liquid storage and liquid assist by exchanging "cold" between at least two different cryogenic liquids, e.g. independently from the main heat exchange line of the air fractionation and/or by using external alternating storage systems
    • F25J3/04509—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages for compensating variable air feed or variable product demand by alternating between periods of liquid storage and liquid assist by exchanging "cold" between at least two different cryogenic liquids, e.g. independently from the main heat exchange line of the air fractionation and/or by using external alternating storage systems within the cold part of the air fractionation, i.e. exchanging "cold" within the fractionation and/or main heat exchange line
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J2200/00—Processes or apparatus using separation by rectification
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J2200/52—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the high pressure column of a double pressure main column system
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    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
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    • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
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    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
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    • F25J2220/42—Separating low boiling, i.e. more volatile components from nitrogen, e.g. He, H2, Ne
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    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10S62/00—Refrigeration
    • Y10S62/901—Single column
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    • Y10S62/00—Refrigeration
    • Y10S62/912—External refrigeration system
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10S62/00—Refrigeration
    • Y10S62/939—Partial feed stream expansion, air

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Description

Die Erfindung betrifft ein Verfahren zur Herstellung von gasförmigem Stickstoff unter niedrigem oder mittlerem Druck in einer Destillationskolonne, ausgehend von einem zu behandelnden Gemisch, das wie Luft im wesentlichen Stickstoff und Sauerstoff enthält.The invention relates to a process for producing gaseous nitrogen under low or medium pressure in a distillation column, starting from a mixture to be treated which, like air, essentially contains nitrogen and oxygen.

Zur Herstellung von Stickstoff aus atmosphärischer Luft beschreibt beispielsweise die US-A-4 662 917 ein Verfahren, bestehend ausFor the production of nitrogen from atmospheric air, US-A-4 662 917, for example, describes a process, consisting of

a) Verdichten des zu behandelnden Gemischs auf einen Druck, der zumindest gleich dem Betriebsdruck der Kolonne ist, in der Größenordnung von 3 bis 5 bar;a) compressing the mixture to be treated to a pressure at least equal to the operating pressure of the column, in the order of 3 to 5 bar;

b) Abkühlen des verdichteten Gemischs in einem Austauscher und Entspannen eines ersten Anteils des abgekühlten Gemischsin einer Turbine, um die für das Verfahren notwendige Kälte zu erzeugen, und anschließend Ausführen der Destillation des Gemischs in der Kolonne, um im oberen Teil der Kolonne einen mit Stickstoff angereichterten Anteil zu erhalten, der anschließend erwärmt wird;b) cooling the compressed mixture in an exchanger and expanding a first portion of the cooled mixture in a turbine in order to generate the cold necessary for the process and then carrying out the distillation of the mixture in the column in order to obtain a nitrogen-enriched portion in the upper part of the column which is subsequently heated;

c) Entnehmen eines Teils des mit Stickstoff angereicherten, erwärmten Anteils als Produkt;c) removing part of the nitrogen-enriched, heated portion as a product;

d) Verdichten eines restlichen Teils des mit Stickstoff angereicherten, erwärmten Anteils und anschließend Abkühlen desselben;d) compressing a remaining part of the nitrogen-enriched, heated portion and then cooling it;

e) Zurückführen eines Teils des genannten restlichen Teils des mit Stickstoff angereicherten Anteils in den unten in der Kolonne gelegenen Austauscher-Verdampfer, in dem dieser Teil in Form einer Flüssigkeit, die reich an Stickstoff ist, kondensiert und die für die Verdampfung in der Kolonne notwendige Wärme liefert;e) returning part of the remaining nitrogen-enriched portion to the exchanger-evaporator located at the bottom of the column, in which part condenses in the form of a liquid rich in nitrogen and supplies the heat necessary for evaporation in the column;

f) Einleiten eines Teils der im vorstehenden Schritt e) kondensierten Flüssigkeit, die reich an Stickstoff ist, in den oberen Teil der Kolonne als zusätzliche Rückflußflüssigkeit;f) introducing a portion of the liquid rich in nitrogen condensed in step e) above into the upper part of the column as additional reflux liquid;

g) Entnehmen eines mit Stickstoff angereicherten Anteils in flüssiger Form aus dem unteren Teil der Kolonne und Entspannen zumindest eines Teils des genannten Anteils auf einen Druck, der geringer ist als der Druck der Kolonne, und Verdampfen dieses Teils in Wärmeaustausch mit dem mit Stickstoff angereicherten Anteil&sub1; der im oberen Teil der Kolonne kondensiert.g) withdrawing a nitrogen-enriched portion in liquid form from the lower part of the column and reducing at least part of said portion to a pressure lower than the pressure of the column and evaporating this portion in heat exchange with the nitrogen-enriched portion₁ which condenses in the upper part of the column.

Die Erfindung hat ein Verfahren nach vorstehender Definition zum Ziel, das gleichzeitig einen hohen Stickstoffentnahmeertrag und ein Halten der Kälte der Vorrichtung mittels Entspannung eines sauerstoffarmen Gases in einer Turbine gestattet.The invention aims to provide a process as defined above which simultaneously allows a high nitrogen extraction yield and maintaining the coldness of the device by expanding a low-oxygen gas in a turbine.

Das Verfahren nach der Erfindung ist dadurch gekennzeichnet, daß es den Schritt Entnehmen des genannten, im Schritt g) verdampften Teils aus dem Kopf der Kolonne als Restgas und Vereinigen desselben mit dem in der Turbine entspannten Gemisch vor dem Einleiten in den Austauscher umfaßt, und daß nur ein zweiter, nicht entspannter Anteil des Gemischs in der Kolonne destilliert wird.The process according to the invention is characterized in that it comprises the step of removing the said part evaporated in step g) from the top of the column as residual gas and combining it with the mixture expanded in the turbine before introducing it into the exchanger, and that only a second, non-expanded portion of the mixture is distilled in the column.

Nach der Erfindung ist die für das Verfahren erforderliche Kälteproduktion zumindest teilweise gewährleistet:According to the invention, the cold production required for the process is at least partially ensured:

- durch Entspannen zumindest eines gasförmigen Kältemittelstroms, der das zu behandelnde Gemisch darstellt, das auf den Druck des Restgases entspannt und mit diesem vermischt wird.- by expanding at least one gaseous refrigerant stream, which represents the mixture to be treated, which is expanded to the pressure of the residual gas and mixed with it.

Die Kälteproduktion kann auch durch Entspannung eines Anteils des rückgeführten Stickstoffs, der dann erwärmt und wieder verdichtet wird, auf einen Druck kleiner oder gleich dem niedrigen Druck gewährleistet werden.The production of cold can also be ensured by expanding a portion of the recycled nitrogen, which is then heated and recompressed to a pressure less than or equal to the low pressure.

Ein kondensierter Teil des Kreisgases kann zu einem Zwischenspeicher mit Entnahme und Wiedereinleiten in die Kolonne im Fall einer Erhöhung des Produktionsstickstoff stroms umgeleitet werden, während ein Teil des sauerstoffreichen Flüssigkeitsstroms zu einem Zwischenspeicher geleitet wird, um im Fall einer Abnahme des gasförmigen Produktionsstickstoffs in den Kondensator im Kopf der Kolonne wieder eingeleitet zu werden, was den erneuten Aufbau des unter Druck stehenden Flüssigstickstoffvorrats gestattet.A condensed portion of the cycle gas can be diverted to an intermediate storage facility for withdrawal and reintroduction into the column in the event of an increase in the production nitrogen flow, while a portion of the oxygen-rich liquid flow is diverted to an intermediate storage facility for reintroduction into the condenser at the top of the column in the event of a decrease in the gaseous production nitrogen, allowing the pressurized liquid nitrogen supply to be rebuilt.

Bei einer speziellen Ausführungsform werden die zwei Arten der Kälteproduktion durch Entspannung des rückgeführten Gases gekoppelt.In a special embodiment, the two types of cold production are coupled by expanding the returned gas.

Die Erfindung wird nun anhand der Zeichnung beschrieben; die Figuren 1 und 2 zeigen unterschiedliche Ausführungsformen des Verfahrens nach der Erfindung.The invention will now be described with reference to the drawing; Figures 1 and 2 show different embodiments of the method according to the invention.

Gemäß Figur 1 wird ein Gasstrom 1, z.B. Luft, auf einen Druck oberhalb des niedrigen Drucks der nachstehend definierten Destillationskolonne 4 verdichtet (nicht dargestellt) und auf übliche Weise gereinigt.According to Figure 1, a gas stream 1, e.g. air, is compressed to a pressure above the low pressure of the distillation column 4 defined below (not shown) and purified in the usual way.

In dem Wärmeaustauscher 2 wird der Strom 1 bis auf eine durch das Niveau 2a dargestellte Zwischentemperatur abgekühlt. Dann wird der gasförmige Strom in der Turbine 3 auf den niedrigen Druck der Größenordnung zwischen 3 und 5 bar absolut entspannt, während ein nichtentspannter Teil des gasförmigen Stroms seine Abkühlung mit den Destillationsprodukten fortsetzt und in die Destillationskolonne 4 auf einem Zwischenniveau zwischen zwei Destillationsböden, dem oberen 4a und dem unteren 4b, eingeleitet wird.In the heat exchanger 2, the stream 1 is cooled to an intermediate temperature represented by the level 2a. Then the gaseous stream is expanded in the turbine 3 to the low pressure of the order of between 3 and 5 bar absolute, while a non-expanded part of the gaseous stream continues its cooling with the distillation products and is introduced into the distillation column 4 at an intermediate level between two distillation trays, the upper 4a and the lower 4b.

Im unteren Teil der Kolonne 4 wird ein sauerstoffangereicherter, flüssiger Anteil gesammelt, der der Kolonne entnommen, in dem Ventil 8 entspannt und schließlich in den Kondensator der Kolonne 4 eingeleitet wird, der im wesentlichen aus einem Austauscher 5 zur Kondensation der Gesamtheit oder eines Teils des gasförmigen, im Kopf der Kolonne 4 verfügbaren Anteils besteht. Dieser sauerstoffangereicherte Anteil wird dem vorstehend genannten Kondensator in Form eines Stroms 9 entnommen, der mit einem Teil des entspannten, gasförmigen Stroms 112 vermischt, in dem Austauscher 2 erwärmt und schließlich verwendet oder am Auslaß des Austauschers 2 entnommen wird.In the lower part of the column 4, an oxygen-enriched liquid fraction is collected, which is withdrawn from the column, expanded in the valve 8 and finally introduced into the condenser of the column 4, which essentially consists of an exchanger 5 for condensing all or part of the gaseous fraction available at the top of the column 4. This oxygen-enriched fraction is withdrawn from the above-mentioned condenser in the form of a stream 9 which is mixed with a part of the expanded gaseous stream 112, heated in the exchanger 2 and finally used or withdrawn at the outlet of the exchanger 2.

Was den im Kopf der Kolonne 4 verfügbaren, stickstoffreichen Anteil betrifft, gewährleistet ein in dem Austauscher 5 kondensierter Teil einen Teil des Rückflusses der Destillation. Ein Teil kann in flüssiger Form über die Leitung 12 entnommen werden. Ein anderer Teil wird gasförmig über die Leitung 11 entnommen. Der entsprechende Strom wird in dem Austauscher 2 erwärmt, um am Auslaß von diesem einen relativ reinen, gasförmigen Stickstoffstrom unter dem niedrigen Druck zu erhalten, wovon ein Teil (X und/oder Y) das mittels der Zerlegungseinheit hergestellte Produkt darstellt.As for the nitrogen-rich fraction available at the top of the column 4, a part condensed in the exchanger 5 ensures part of the reflux of the distillation. One part can be taken in liquid form via line 12. Another part is taken in gaseous form via line 11. The corresponding stream is heated in the exchanger 2 in order to obtain, at the outlet thereof, a relatively pure gaseous nitrogen stream at low pressure, part of which (X and/or Y) represents the product produced by means of the separation unit.

Ein anderer, in 13 verdichteter Teil dieses Stroms 11, der den Fluß 14 bildet, wird in die Zerlegungseinheit rückgeführt. Der Strom 14 wird zuerst in dem Austauscher 2 abgekühlt und zumindest teilweise in dem Austauscher 6 im unteren Teil der Kolonne 4 durch Wärmeaustausch mit dem säuerstoffreichen Anteil während dessen Verdampfung kondensiert. Dann wird der kondensierte Stickstoffstrom 20 in dem Ventil 17 entspannt und in den Kopf der Kolonne 4 eingeleitet.Another part of this stream 11, compressed in 13 and forming the flow 14, is returned to the separation unit. The stream 14 is first cooled in the exchanger 2 and at least partially in the exchanger 6 in the lower part of the column 4 by heat exchange with the oxygen-rich portion during its evaporation. The condensed nitrogen stream 20 is then expanded in the valve 17 and introduced into the top of the column 4.

In dieser ersten Ausführungsform arbeitet die Destillationskolonne 4 unter einem relativ niedrigen Druck von beispielsweise zwischen 3 und 5 bar absolut.In this first embodiment, the distillation column 4 operates under a relatively low pressure of, for example, between 3 and 5 bar absolute.

Im übrigen können die in der Anordnung verfügbaren, flüssigen Anteile während der Perioden mit relativ geringer Produktion gespeichert und diese flüssigen Anteile während der Perioden mit hoher Produktion in die Vorrichtung rückgeführt werden.Furthermore, the liquid portions available in the device can be stored during periods of relatively low production and these liquid portions can be returned to the device during periods of high production.

Zu diesem Zweck kann der rückgeführte Stickstoffstrom über eine Leitung 20a zu einem Zwischenspeicher 20c geleitet und über eine Leitung 20b stromab von dem Ventil 17 in die Kolonne 4 zurückgeführt werden. Auf die gleiche Weise kann der sauerstoffreiche Anteil 7 der Vorrichtung über eine Umgehungsleitung 7a zu dem Zwischenspeicher 7c geleitet und über eine Leitung 7b stromab von dem Ventil 8 in die Kolonne 4 zurückgeführt werden.For this purpose, the recirculated nitrogen stream can be passed via a line 20a to an intermediate storage 20c and returned to the column 4 via a line 20b downstream of the valve 17. In the same way, the oxygen-rich portion 7 of the device can be passed via a bypass line 7a to the intermediate storage 7c and returned to the column 4 via a line 7b downstream of the valve 8.

Die Ausführungsform in Figur 2 unterscheidet sich von der in Figur 1 dargestellten durch folgende Merkmale:The embodiment in Figure 2 differs from that shown in Figure 1 by the following features:

- ein erster Teil la der verdichteten Luft 1 wird in dem Austauscher 2 abgekühlt und dann bei 121 in die Kolonne 4 eingeleitet;- a first portion la of the compressed air 1 is cooled in the exchanger 2 and then introduced into the column 4 at 121;

- der andere Teil 1b der verdichteten Luft 1 wird vor seinem Eintritt in den Austauscher 2 umgeleitet, strömt dann in den Verdichterteil 50 einer aus einer Turbine 3 und einem Booster 50 bestehenden Einheit, wird in dem Austauscher 51 bis auf Umgebungstemperatur abgekühlt und danach in den Austauscher 2 eingeleitet und anschließend bei einer Zwischentemperatur entnommen, in der Turbine 3 bei 112 entspannt, mit dem sauerstoffreichen Anteil 9 zusammengeführt und in dem Kondensator 5 verdampft.- the other part 1b of the compressed air 1 is diverted before entering the exchanger 2, then flows into the compressor part 50 of a unit consisting of a turbine 3 and a booster 50, is cooled in the exchanger 51 to ambient temperature and then introduced into the exchanger 2 and subsequently removed at an intermediate temperature, expanded in the turbine 3 at 112, combined with the oxygen-rich portion 9 and evaporated in the condenser 5.

Die zwei anhand der Figuren 1 und 2 beschriebenen, umschaltbaren Ausführungsformen haben den Vorteil, daß eine Produktion von gasförmigem Stickstoff möglich ist, die zwischen 50 und 150 % der Nennproduktion liegen kann.The two switchable embodiments described with reference to Figures 1 and 2 have the advantage that a production of gaseous nitrogen is possible which can be between 50 and 150% of the nominal production.

Claims (1)

1. Verfahren zur Herstellung von gasförmigem Stickstoff ausgehend von einem in einer Destillationskolonne (4) zu behandelnden Gemisch, wobei das Gemisch insbesondere Stickstoff und Sauerstoff umfaßt und das Verfahren aus den folgenden Schritten besteht:1. Process for producing gaseous nitrogen starting from a mixture to be treated in a distillation column (4), the mixture comprising in particular nitrogen and oxygen and the process consisting of the following steps: a) Verdichten des zu behandelnden Gemischs auf einen Druck, der zumindest gleich dem Betriebsdruck der Kolonne ist, in der Größenordnung von 3 bis 5 bar;a) compressing the mixture to be treated to a pressure at least equal to the operating pressure of the column, in the order of 3 to 5 bar; b) Abkühlen des verdichteten Gemischs in einem Austauscher (2) und Entspannen eines ersten Anteils des abgekühlten Gemischs in einer Turbine (3), um die für das Verfahren notwendige Kälte zu erzeugen, und anschließend Ausführen der Destillation des Gemischs in der Kolonne, um im oberen Teil der Kolonne einen mit Stickstoff angereicherten Anteil zu erhalten, der anschließend erwärmt wird;b) cooling the compressed mixture in an exchanger (2) and expanding a first portion of the cooled mixture in a turbine (3) in order to generate the cold necessary for the process and then carrying out the distillation of the mixture in the column in order to obtain a nitrogen-enriched portion in the upper part of the column, which portion is subsequently heated; c) Entnehmen eines Teils des mit Stickstoff angereicherten, erwärmten Anteils als Produkt;c) removing part of the nitrogen-enriched, heated portion as a product; d) Verdichten eines restlichen Teils des mit Stickstoff angereicherten, erwärmten Anteils und anschließend Abkühlen desselben;d) compressing a remaining part of the nitrogen-enriched, heated portion and then cooling it; e) Zurückführen eines Teils des genannten restlichen Teils des mit Stickstoff angereicherten Anteils in den unten in der Kolonne gelegenen Austauscher-Verdampfer (6), in dem dieser Teil in Form einer Flüssigkeit, die reich an Stickstoff ist, kondensiert und die für die Verdampfung in der Kolonne notwendige Wärme liefert; f) Einleiten eines Teils der im vorstehenden Schritt e) kondensierten Flüssigkeit, die reich an Stickstoff ist, in den oberen Teil der Kolonne als zusätzliche Rückflußflüssig keit;e) returning a portion of said remaining portion of the nitrogen-enriched fraction to the exchanger-evaporator (6) located at the bottom of the column, in which said portion condenses in the form of a liquid rich in nitrogen and supplies the heat necessary for evaporation in the column; f) introducing a portion of the liquid rich in nitrogen condensed in step e) above into the upper part of the column as additional reflux liquid; g) Entnehmen eines mit Sauerstoff angereicherten Anteils in flüssiger Form aus dem unteren Teil der Kolonne und Entspannen zumindest eines Teils des genannten Anteils auf einen Druck, der geringer ist als der Druck der Kolonne, und Verdampfen dieses Teils im Wärmetausch mit dem mit Stickstoff angereicherten Anteil, der im oberen Teil der Kolonne kondensiert; und dadurch gekennzeichnet, daß das Verfahren den folgenden Schritt umfaßt:g) withdrawing an oxygen-enriched fraction in liquid form from the lower part of the column and depressurizing at least part of said fraction to a pressure lower than the pressure of the column and evaporating this fraction in heat exchange with the nitrogen-enriched fraction condensing in the upper part of the column; and characterized in that the process comprises the following step: h) Entnehmen des genannten im Schritt g) verdampften Teils aus dem Kopf der Kolonne (4) als Restgas und Vereinigen desselben mit dem in der Turbine (3) entspannten Gemisch und Einleiten in den Austauscher (2), und daß nur ein zweiter, nicht entspannter Anteil des Gemischs in der Kolonne destilliert wird.h) removing the part evaporated in step g) from the top of the column (4) as residual gas and combining it with the mixture expanded in the turbine (3) and introducing it into the exchanger (2), and that only a second, non-expanded portion of the mixture is distilled in the column. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der als Produkt entnommene Stickstoff in gasförmiger und/oder flüssiger Form vorliegt.2. Process according to claim 1, characterized in that the nitrogen removed as a product is in gaseous and/or liquid form. 3. Verfahren nach einem der Ansprüche 1 und 2, bestehend aus dem Nachverdichten eines ersten Anteils des verdichteten Gemischs in einem Verdichter (50), der durch die Turbine (3) angetrieben wird, und dem Abkühlen des ersten nachverdichteten Anteils und Entspannen desselben in der Turbine (3).3. Method according to one of claims 1 and 2, consisting of recompressing a first portion of the compressed mixture in a compressor (50) which is driven by the turbine (3), and cooling the first recompressed portion and relaxing it in the turbine (3). 4. Verfahren nach einem der Ansprüche 1 bis 3, bei dem der erste Anteil des Gemischs in der Turbine (3) auf einen Druck nahe dem Atmosphärendruck entspannt wird.4. Method according to one of claims 1 to 3, in which the first portion of the mixture in the turbine (3) is expanded to a pressure close to atmospheric pressure. -5. Verfahren nach einem der Ansprüche 1 bis 4, bei dem ein kondensierter Teil (20a) des mit Stickstoff angereicherten Anteils aus dem Schritt e) zu einem Kapazitätspuffer (20c) umgeleitet wird, wenn die Produktion von gasförmigem Stickstoff reduziert ist.-5. A method according to any one of claims 1 to 4, wherein a condensed portion (20a) of the nitrogen-enriched portion from step e) is diverted to a capacity buffer (20c) when the production of gaseous nitrogen is reduced. 6. Verfahren nach Anspruch 5, bei dem ein Teil des mit Sauerstoff angereicherten Anteils aus dem Schritt g) zu einem Kapazitätspuffer (7c) umgeleitet wird, wenn die Produktion von gasförmigem Stickstoff maximal ist.6. The method according to claim 5, wherein a part of the oxygen-enriched portion from step g) is diverted to a capacity buffer (7c) when the production of gaseous nitrogen is at a maximum.
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US5373699A (en) 1994-12-20

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